Evidence abounds that LSD continues to be a significant drug of abuse. Unfortunately, existing GC/MS tests for LSD are generally unable to detect the drug in urine for more than a few hours after ingestion. Consequently, there is a critical need for development of a more sensitive confirmation assay. It is proposed to develop such an assay through use of a tandem mass spectrometer (Finnigan MAT TSQ-70). Research will include investigation of methods for extraction of LSD and its metabolites, derivitization, sample introduction into the tandem mass spectrometer, and methods of ionization and mass analysis. Urine samples fortified with known concentrations of LSD and one of its metabolites, N-demethyl LSD, as well as submitted urine specimens that have tested positive for LSD by a radioimmunoassay, will be analyzed in order to determine the new assay's limit of quantitation, precision, accuracy, and dynamic range.